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By R. W. Van Dolah

An investigation was made of the distances over which sympathetic detonation of ammonium nitrate (AN) and ammonium nitrate-fuel oil (AN-FO) might be expected. Large-scale gap tests used two types of AN-FO donor charges in three sizes with AN, both at ambient and elevated temperatures, and AN-FO acceptor charges. Donor sizes were varied to test the validity of a scaling law commonly used in quantity distance tables. The up-and-down experimental design was chosen to determine the 50-percent initiation point efficiently. The acceptor charges were instrumented to indicate initiation and to determine detonation velocity. Other electronic techniques for measuring the rate of growth, stability of detonation, and detonation pressures were employed. Air shock and fragment velocities between charges were measured by electronic and photographic methods, and determination of side-on air-blast pressures and impulse duration were made for about half the shots. Separation distances between donor and acceptor were found to be larger than anticipated both for the AN and the AN-FO. With AN-FO acceptors and a 16-gage steel faced donor, one initiation occurred at a separation of 53 feet or nearly 16-charge diameters; with AN, initiation occurred at 4 to 5-1/2- charge diameters.

Jan 1, 1966

By Galen G. Waddell

Dilation and contraction of the rock surrounding horizontal access open-ings of a deep mine were analyzed during stope advance to determine what type of measurements, made with relatively inexpensive instrumentation, would best reflect the rock behavior. A variety of instruments, mostly mechanical extensometers, were used. Detailed descriptions are given of Down-the-hole extensometers, floating rockbolt clusters, transit surveys, and other instruments and measuring techniques. Although all of the radial-deformation-rate graphs illustrated useful rock behavior data, the most informative graphs were compiled from data procured with the radial extensometers that penetrated, to various depths, the rock around the access openings. An analysis is given of measurement data on the rock around lateral drifts and across and adjacent to the nearly vertical vein of the Star mine, Burke, Idaho. Several useful relationships were found between the rock deformation rate and the stoping process. Information was produced on the elastic state of rock around an underground opening, effectiveness of stope support, rheology of rock, zone of influence around stopes, effectiveness of rockbolts, axis of maximum strain in a plane perpendicular to the long axis of the lateral, and other phenomena. This information could be of particular value in determining location, design, and support of underground openings.

Jan 1, 1966

By L. J. E. Hofer

The Bureau of Mines determined rates of adsorption and desorption of methane as a function of particle size and temperature, using coals from the Pocahontas No.3 seam (lvb) from the Bishop mine of western Virginia, and the Pittsburgh seam (hvab) from the Pursglove No. 15 mine of northern West Virginia. For a given coal sample and temperature, the rate curves for adsorption and desorption are essentially the same when expressed on a fractional approach to equilibrium basis. The rates of adsorption and desorption increased eightfold as the particle size was decreased from 6-8 to 270-325 mesh per inch. The adsorption process appears to be diffusion controlled. Rate of sorption processes increased with increasing temperature; however, the amount adsorbed at equilibrium decreased.

Jan 1, 1966

By J. W. Town

The Bureau of Mines conducted petrographic classification and flotation studies to determine if acid-grade concentrates could be obtained from individual and composite samples from the Meade Peak member of the Phosphoria Formation, Idaho. The petrographic studies were made to determine the effect of compositional features on concentration of phosphates. The ore grade, ovule size, and clay content were the main features affecting grade and recovery of phosphate. Flotation results on roasted ore with a tall oil emulsion scheme showed that beds containing over 10 percent P2O5 could be beneficiated and composited with the two high-grade beds to produce a composite concentrate containing 31.9 percent 05 at 84.3 percent recovery. Treatment of these intermediate-grade phosphate beds by flotation increased ore reserves over 200 percent and increased the ore-to-waste ratio in the ore zone from 1:5.7 to 1:0.27.

Jan 1, 1966

By R. L. Benner

The Bureau of Mines investigated the ZnO-Fe2O3-Fe3O4 system at 1,000°, 1,300°, and 1,400° C, with oxygen pressures between 1.0 and lx10-4 atmospheres. The results, divided into the thermodynamic properties as related to the spinel structure, and the thermodynamic properties as related to zinc concentrate roasting, were used to calculate the activities of ZnO, Fe2O4, and Fe3O4 within the spinel solid solution region of the ternary system, and the pseudo-binary activities of ZnFe2O4 and Fe304. The activities of both systems show large positive deviations from Raoult's Law, especially at high Fe3O4 concentrations. The free energies, the enthalpies, and the entropies of mixing for the binary system were calculated from the binary activities, and the entropies of mixing were compared with two statistical models, one representing an ideal solution, and one representing the mixing of a normal with an inverse spinel. The binary entropy of mixing seemed to be better represented by the latter statistical model, indicating that the tetrahedral and octahedral cations of the reactants tend to remain in the product, even at the high temperatures of the study. This comparison also indicated that the cations of the components are the major contributing factors to the thermodynamic properties.

Jan 1, 1966

By Harry R. Johnson

Laboratory experiments were conducted to study the carbon deposition characteristics of a high-gravity, paraffin-base crude oil. The results of these experiments indicate that a fuel supply adequate to initiate a combustion wave can be deposited in high-gravity-oil reservoirs. These results are significant because there has been considerable doubt whether oils over 35° API gravity are able to deposit sufficient fuel. Considered in these studies were the effects of air flux, temperature, initial oil saturation, and time on carbon deposition. Conditions that maximized carbon deposition in the laboratory and an understanding of the nature of carbon formation are shown by graphical interpretation of the data. Statistical techniques were used to design and analyze the results of the retort tests. For the same amount of laboratory work, this approach yields more information about the systems that were studied than the classical method of research presently used in many laboratories. In addition, the accuracy of calculating the effect of each variable on carbon deposition is twice that of the classical approach. This paper develops the statistical approach to research without complex mathematics, thus enabling the reader to grasp the concept of how statistics can be applied to study many complicated problems.

Jan 1, 1966

By Jack G. Croeni

A study was made by the Bureau of Mines to determine the influence of high energy-rate deformation on the structures and properties of low-carbon steel, stainless steel, titanium, titanium-6 percent aluminum-4 percent vanadium, beryllium, molybdenum, and tungsten. The purpose of this study was to determine relative formability, the effect of energy and temperature on metalworking parameters and resulting structures, and the properties of materials formed by this technique. Forming techniques were limited to upset forging and direct extrusion on pneumatic-mechanical forming machines. Results show that considerable grain refinement can be achieved by careful control of deformation and forming temperature by high energy-rate techniques. Significant improvements in strength were observed as a result of this refined structure. Approximate deformation resistance as a function of temperature was determined for a variety of materials.

Jan 1, 1966

By Robert S. Warfield

Eight samples of high-volatile bituminous coal, each large enough for a study of its coking properties by the Bureau of Mines, were obtained from a location along the Kukpowruk River, Arctic Northwestern Alaska. Bench scale and pilot plant carbonization studies with several patterns of coal blending were conducted. The data from these tests were compared to data from similar tests on a coking blend used by the Kaiser Steel Corporation at Fontana, Calif. The majority of the samples representing the 20-foot seam was found to have significant coking properties, and produced coke approaching metallurgical quality when blended with selected coking coals. Although oxidation effects were evident in the samples representing upper portions of the seam, it appears that the whole seam could be used.

Jan 1, 1966

By R. W. Van Dolah

An attempt has been made in this investigation to define the conditions under which ammonium nitrate (AN) might detonate as a result of involvement in fire. The initiation of detonation by shocks derived from explosives or from projectile impact was investigated as a function of temperature and charge diameter. A new technique was devised to investigate the burning of raw and contaminated AN under pressure. No transition, to detonation in AN was obtained in the burning experiments. The critical diameter for detonation of fertilizer-grade AN was found to be quite small when the AN was at temperatures just below melting point; this indicates that initiation of detonation may be less difficult at elevated temperatures but such initiation by gas-phase detonation was shown to be unlikely. Transition from burning to detonation was obtained with AN intimately mixed with fuels that included polyethyl-ene, paper, and fuel oil when these were contained in vessels with restricted vents. However, the experimental results supported by an analytical study indicate that the initiation of detonation in AN from fire exposure in normal storage and from transportation incidents is quite improbable. The detonation of AN in recent incidents more likely may have resulted from the effects of adjacent explosions.

Jan 1, 1966

By James F. Devine

The radial, vertical, and transverse components of particle velocity were recorded by Bureau of Mines investigators along gage arrays extending in one or two directions for 145 to 3,170 feet at five quarries. Of the 39 quarry blasts, 12 were instantaneous blasts, 5 were of the one hole per delay type, using millisecond delayed caps, and 22 were multiple hole per delay type employing millisecond delay detonating fuse connectors. Charge weight per hole ranged from 8 to 1,500 pounds, and the charge weight per delay interval, including the instantaneous blasts, ranged from 25 to 4,620 pounds.

Jan 1, 1966

By P. L. Weston

The Bureau of Mines used high-temperature reduction roasting, magnetic separation, acid-leaching, and autoclave precipitation processes to recover iron and manganese from brown Cuyana range ores of Minnesota. Wet magnetic separation concentrated over 90 percent of the iron in 3 of 4 ores as high grade products analyzing 74 to 85 percent iron, 2.5 to 6 percent manganese, and 3 to 10 percent SiO2. The nonmagnetic fractions were leached with dilute sulfuric acid extracting 83 to 93 percent of the contained manganese and small amounts of iron. The leach solutions contained Mn-to-Fe and Mn-to-SiO2 ratios favorable enough for possible consumption in metallurgical mane operations. Exceptionally pure Mn solutions were achieved by pressure precipitation of the remaining iron in an autoclave followed by lime precipitation of silica and alumina.

Jan 1, 1966

By H. R. Babitzke

To develop alloys suitable for use at elevated temperatures, columbium and tantalum were combined with tungsten, hafnium, vanadium, zirconium, and titanium, and the resulting alloys were evaluated with respect to fabricability, hardness, Electrical resistivity, strength at elevated temperatures, oxidation resistance, and bend transition. Of the 23 compositions tested, Cb-2OHf-5W-10Ti exhibited superior high-temperature properties. A recrystallized sample of this alloy was fabricable at room temperature, had a strength of 44,000 psi at 1,200° C, and had an oxidation rate of only 7.7 mg/cm2/hr at 1,000° C.

Jan 1, 1966

By Jr. Hazen

This report documents 653 sets of sample data involving 78,366 assays obtained from past exploration for various minerals and metals. Most of these data have been taken from published reports describing exploration projects, conducted jointly by the Bureau of Mines and the Geological Survey, for the Strategic Minerals Program from 1940 through 1949. Means and standard deviations have been computed for the exploration assay data and have been plotted on graphs for 22 minerals and metals. A mathematical model, based on the binomial distribution, has been developed to explain the configuration of the plots of the exploration means and standard deviations. The two statistics, mean and standard deviation, which describe assay data, have been used for simulating probability models. These probability models then have been combined with the binomial model of the exploration assays and related to the sequential decision process associated with exploration drilling for mineral deposits. These probability regions can be used to form the basis for sequentially predicting the probable range of the average grade of mineral or metal that may be expected as an exploration drilling program is continued after the initial discovery of mineralization has been made.

Jan 1, 1966

By C. I. Pierce

The Bureau of Mines used an electrolytic tank model to investigate the response of guard electrodes of different dimensions under different simulated reservoir conditions. Sandstone disks from the Berea and Connellsville Formations were used as resistive beds in the model, and agar gel or water was used as conductive beds. In the experiments, bed thickness, hole diameter, mud resistivity, and bed resistivity were varied. The guard electrode is an excellent tool for determining true bed resistivity in the thin-bedded oil reservoirs of the Appalachian area. Vertical resolution and resistivity values are good when there is little or no invasion. Resistivity values are near true bed resistivity in beds thicker than about six hole diameters when the electrode-to-hole-diameter ratio is close to 1. However, low-resistivity muds cause false peaks to appear on the logs near bed boundaries in thick beds, and for resistive beds having a thickness approximately three to five times the hole diameter, apparent resistivities tend to be excessively high when mud resistivity is low.

Jan 1, 1966

By P. C. Good

Work was done to determine conditions necessary for efficient electrodeposition of aluminum from fused chloride electrolytes. Aluminum was deposited from a molten chloride salt electrolyte over a temperature range of 150° to 750° C. At lower temperatures in a heat-resistant glass cell, aluminum was deposited on stainless steel and on aluminum cathodes. The deposit was recovered in the form of light, feathery dendrites that could not be consolidated. At 750° C, molten aluminum was deposited at cathode current efficiencies as high as 90 to 100 percent on titanium diboride cathodes and in molten aluminum cathodes. Nitride-bonded silicon carbide was the best cell material, although porcelain was also used. The electrolyte consisted of a mixture of sodium and potassium chlorides in 1 to 1 mole ratio, containing aluminum chloride in concentrations ranging from 2 to 30 weight-percent in cells holding up to 1,000 grams of electrolyte. Generally favorable results were attained in studies made at temperatures greater than the melting point of aluminum.

Jan 1, 1966

By Paul V. Mullins

Review and evaluation of all available data on the vapor pressure of car-bon dioxide at the ice point, including previously unpublished results obtained by the Bureau of Mines, are presented. Suggested corrections and adjustments to all the data yield an average value of 26,136.4 mm mercury. Indicated agreement is within plus 1 part in 8,000 to minus 1 part in 11,000. A novel pressure bomb in which a sample of pure carbon dioxide is placed and sealed by a diaphragm fluid separator and its use as a reference pressure standard for extended and repeated use in the calibration of deadweight gages is described.

Jan 1, 1966

By H. C. Fuller

A method was devised and developed by the Bureau of Mines for decomposing manganese sulfate at significantly lower temperature than that required by the conventional procedure of using heat alone. This technique, called the partial reduction method, effected decomposition at 700° to 800° C, as compared to 900° 1,000° C normally required. The process consisted of heating, in the absence of oxygen, a mixture of manganese sulfate and a controlled quantity of a reducing agent. The suitability of commercial-type equipment was tested in laboratory-size models of an externally heated rotary kiln, a r bbled muffle-hearth furnace, and a fluidized-bed reactor. The rabbled-hearth furnace gave the best results with the least operating difficulty produced a gas containing more than 80 percent SC and eliminated 96 percent of the sulfur when coal was used as the reductant. Sintering of the powdery decomposition product produced an agglomerate containing, in percent, 63.6 Mn and 0.4 S.

Jan 1, 1966

By Leo A. Schrider

This report analyzes the successful low-pressure gas drive in the Keener sand of the Bonds Creek oilfield, Pleasants and Ritchie Counties, W. Va.) and predicts its future performance. Core analysis from two wells and electrical and radioactivity logs were used to evaluate the reservoir characteristics. Production records over a 37-year period indicate that over 240,000 barrels of oil have been produced from the Keener sand by low-pressure gas injection. Decline-curve analysis shows that 165,000 additional barrels should be recovered from 108 acres of productive sand by continuing this secondary-recovery method.

Jan 1, 1966

By Charles M. Mason

The Bureau of Mines evaluated equipment and procedures for drop-weight testing of explosive liquids as prescribed by Test 4) a widely used method. It was demonstrated that partial ignitions, originally designated as negative results, should be designated positives; it was also shown that wear or erosion of the sample cups and the type of mount used for the apparatus had important effects on the results. Relative sensitivity as measured by Test 4 was found to vary slightly with temperature. The Bureau also designed a fixed 2-kg weight and associated electromagnetic release, which subsequently were incorporated as standard in a revision of Test 4. The original concept that the test involves only adiabatic compression was found to be an oversimplification; an alternate mechanism for the initiation process is proposed in which due consideration is given to the effects of cavitation and microjets.

Jan 1, 1966

By A. L. Service

Idaho has nearly 6 billion tons of potential sources of phosphorite, 10 to 31 percent P2O5' above and within 100 feet below entry level, the largest potential of any State in the United States. In 1963 Idaho ranked third after Florida and Tennessee in total mine and marketable production of phosphate rock; Montana ranked fourth. This report describes phosphate deposits, mines, and prospects in 10 districts covering most of the Idaho phosphate field. All mine production of phosphate rock in Idaho comes from surface mines and is processed to phosphate fertilizers, phosphoric acid, and elemental phosphorus. Producing districts are Fort Hall (Gay mine), Trail Creek (Conda and Ballard mines), and Crow Creek (Georgetown Canyon mine). FMC Corp. and J. R. Simplot Co. at Pocatello have the largest elemental phosphorus and fertilizer production facilities, respectively, in the State, followed by Monsanto Co. and El Paso Natural Gas Products Co. (formerly Central Farmers Fertilizer Co.). The only other major phosphate processing plant in the State is the phosphoric acid and phosphate fertilizer complex at Kellogg operated by the Bunker Hill Co. In 1963 a plant was constructed and put on line at Monsanto, Idaho, to recover vanadium from ferrophosphorus produced by electric furnace operations in the area. El Paso Natural Gas Products Co. completed construction of a fertilizer and phosphoric acid plant near Conda in 1965. There is a small fertilizer plant producing phosphate fertilizers for local consumption in Soda Springs.

Jan 1, 1966